A kind of preparation method of 2-arylquinoline derivatives
An arylquinoline and derivative technology, which is applied in the field of preparation of 2-arylquinoline derivatives, can solve the problems of expensive aryl source substrates or catalysts, limited scope of application of substrates, harsh reaction conditions, and the like, Achieving the effect of high yield, easy operation and mild reaction conditions
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Embodiment 1
[0031] Example 1.R 1 =-CH 3 , R 2 = R 3 When =-H, the preparation of 2-phenyl-4-methylquinoline derivatives
[0032] Add 4-methylquinoline (0.5mmol, 71.5mg) and benzoic acid (1.0mmol, 122mg) in a 50mL round bottom flask, then add the catalyst AgNO 3 (0.05mmol, 8.5mg), oxidant K 2 S 2 o 8 (1.5mmol, 405mg), trifluoroacetic acid (0.5mmol, 72mg) as auxiliary agent and 5.0mL acetonitrile as solvent, reflux reaction at 90°C for 8.0h; NaHCO 3 The solution was neutralized to neutral, extracted twice with 15mL ethyl acetate, and the extract was washed twice with saturated brine; the extract was washed with anhydrous Na 2 SO 4 After drying and concentration under reduced pressure, it was separated and purified by column chromatography (eluent: ethyl acetate / petroleum ether=1 / 15) to obtain 0.083 g of a yellow viscous liquid with a yield of 76.0%.
[0033]
[0034] yellow viscous liquid; 1 H NMR (400MHz, CDCl 3 )δ:8.24(d,J H-H =8.4Hz,1H),8.16(d,J H-H =7.2Hz, 1H), 7.75-7.7...
Embodiment 2
[0035] Example 2.R 1 =-CH 3 , R 2 =-H, R 3 =-OCH 3 , the preparation of 2-(4-methoxyphenyl)-4-methylquinoline derivatives
[0036]Add 4-methylquinoline (0.5mmol, 71.5mg) and 4-methoxybenzoic acid (1.0mmol, 152mg) in 50mL round bottom flask, then add catalyst AgNO 3 (0.05mmol, 8.5mg), oxidant K 2 S 2 o 8 (1.5mmol, 405mg), trifluoroacetic acid (0.5mmol, 72mg) as auxiliary agent and 5.0mL water as solvent, reflux reaction at 100°C for 10.0h; after the reaction, add 5.0mL ethyl acetate, then filter to remove insoluble , add saturated NaHCO to the filtrate 3 The solution was neutralized to neutral, extracted twice with 15mL ethyl acetate, and the extract was washed twice with saturated brine; the extract was washed with anhydrous Na 2 SO 4 After drying and concentration under reduced pressure, it was separated and purified by column chromatography (eluent: ethyl acetate / petroleum ether=1 / 15) to obtain 0.097 g of a yellow viscous liquid with a yield of 78.0%.
[0037] ...
Embodiment 3
[0039] Example 3.R 1 =-CH 3 , R 2 =-H, R 3 When =-F, the preparation of 2-(4-fluorophenyl)-4-methylquinoline derivatives
[0040] Add 4-methylquinoline (0.5mmol, 71.5mg) and 4-fluorobenzoic acid (1.0mmol, 140mg) in a 50mL round bottom flask, then add the catalyst AgNO 3 (0.05mmol, 8.5mg), oxidant K 2 S 2 o 8 (1.5mmol, 405mg), trifluoroacetic acid (0.5mmol, 72mg) as auxiliary agent and 3.0mL acetonitrile and 3.0mL water as mixed solvent, reflux reaction at 100°C for 9.0h; after the reaction, add 5.0mL ethyl acetate , and then filtered to remove insoluble matter, and saturated NaHCO was added to the filtrate 3 The solution was neutralized to neutral, extracted twice with 15mL ethyl acetate, and the extract was washed twice with saturated brine; the extract was washed with anhydrous Na 2 SO 4 After drying and concentration under reduced pressure, it was separated and purified by column chromatography (eluent: ethyl acetate / petroleum ether=1 / 10) to obtain 0.089 g of a yel...
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